CN117186832A - Storage-stable one-component dealcoholized organosilicon sealant composition and preparation method thereof - Google Patents
Storage-stable one-component dealcoholized organosilicon sealant composition and preparation method thereof Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 86
- 239000000565 sealant Substances 0.000 title abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 37
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- 239000004590 silicone sealant Substances 0.000 claims abstract description 29
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 15
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 14
- 229910000077 silane Inorganic materials 0.000 claims abstract description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000049 pigment Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 25
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 7
- FIRQYUPQXNPTKO-UHFFFAOYSA-N ctk0i2755 Chemical class N[SiH2]N FIRQYUPQXNPTKO-UHFFFAOYSA-N 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical group CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 5
- 125000003277 amino group Chemical group 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 claims description 2
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- JCGDCINCKDQXDX-UHFFFAOYSA-N trimethoxy(2-trimethoxysilylethyl)silane Chemical compound CO[Si](OC)(OC)CC[Si](OC)(OC)OC JCGDCINCKDQXDX-UHFFFAOYSA-N 0.000 claims description 2
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 claims description 2
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 27
- 239000011248 coating agent Substances 0.000 description 24
- 238000000576 coating method Methods 0.000 description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 17
- 229910052710 silicon Inorganic materials 0.000 description 17
- 239000010703 silicon Substances 0.000 description 17
- 238000009472 formulation Methods 0.000 description 16
- 238000001723 curing Methods 0.000 description 14
- 239000003292 glue Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 11
- 239000007822 coupling agent Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 239000006229 carbon black Substances 0.000 description 8
- 229920001296 polysiloxane Polymers 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 241001247482 Amsonia Species 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000013522 chelant Substances 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 229920002379 silicone rubber Polymers 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
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- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229940083037 simethicone Drugs 0.000 description 4
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- 238000010009 beating Methods 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004026 adhesive bonding Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
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- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- INFDPOAKFNIJBF-UHFFFAOYSA-N paraquat Chemical compound C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 INFDPOAKFNIJBF-UHFFFAOYSA-N 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013006 addition curing Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229920013822 aminosilicone Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000013005 condensation curing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a storage-stable one-component dealcoholized silicone sealant composition and a preparation method thereof, wherein the silicone sealant composition comprises the following components: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, 80-120 parts by weight of calcium carbonate, 0-10 parts by weight of plasticizer, 0-5 parts by weight of pigment and 6-12 parts by weight of curing agent, wherein the curing agent comprises a mixture which is obtained by stirring and mixing (by weight ratio) an alcohol-removing cross-linking agent (5-7) and (1-4) and (0.1-0.8) of a catalyst and a polyamino silane oligomer for 30-60 min under the moisture-isolating condition. The organosilicon sealant composition has good adhesive property and prolonged shelf life.
Description
Technical Field
The invention belongs to the field of organic silicon sealants, and particularly relates to a storage-stable single-component dealcoholized organic silicon sealant composition and a preparation method thereof.
Background
The organic silicon sealant has natural toughness and excellent weather resistance, and is widely used for bonding and sealing in the fields of construction, traffic, electronic and electric appliances, automobiles and the like.
In the field of automobile lamps, the sensory quality of the whole automobile, the using effect of the automobile lamp and even the driving safety are greatly influenced due to the condensation of fog in the automobile lamp, so that various automobile manufacturers currently adopt an anti-fog coating mode to prevent fog condensation. The anti-fog coating has stronger hydrophilicity, and as such, the water vapor in the car lamp can be uniformly spread when condensed when encountering cold, and water drops are not formed, so that the car lamp is not fogged.
However, when the conventional silicone sealant is used for bonding a vehicle lamp, since the excessive crosslinking agent and the residual siloxane rings D3 to D10 are easily volatilized inside the vehicle lamp, the reaction with the anti-fog coating gradually occurs, and as a result, the originally hydrophilic coating becomes hydrophobic, resulting in failure of the anti-fog coating. Failure of the anti-fog coating is one of the difficulties of the organosilicon sealant for bonding the car lamp.
Chinese patent CN 111019593B discloses an equal proportion mixed organic silicon sealant for anti-fog vehicle lamp and its preparation method, wherein the a component of the equal proportion mixed organic silicon sealant for anti-fog vehicle lamp comprises: 100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 20-120 parts of nano active calcium carbonate, 0-10 parts of white carbon black and 0-30 parts of plasticizer 1; the component B comprises: 100 parts of component B base material, 0 to 15 parts of pigment, 0 to 30 parts of plasticizer 2, 3 to 20 parts of cross-linking agent, 1 to 8 parts of coupling agent and 0.01 to 2 parts of catalyst; wherein the base materials of the component B are as follows: 100 parts of plasticizer 3, 80-240 parts of filler and 0-20 parts of white carbon black. Compared with the traditional double-component silicone sealant, the A, B component equal proportion mixed use has the advantages of low requirement on proportioning precision of gluing equipment, high curing speed and no influence on an anti-fog coating in an anti-fog car lamp.
Chinese patent CN 107163908B provides a two-component silicone rubber sealant for automotive lamp assembly sealing, comprising a component a and a component B, wherein the component a is prepared from the following raw materials in parts by weight: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, 0-20 parts by weight of simethicone, 70-120 parts by weight of calcium carbonate and 0-10 parts by weight of white carbon black; the component B is prepared from the following raw materials in parts by weight: 20 to 100 parts of color paste, 8 to 15 parts of cross-linking agent, 5 to 12 parts of coupling agent, 0 to 20 parts of white carbon black and 0.5 to 3 parts of catalyst.
Chinese patent CN 107880841B discloses an anti-fog silicone sealant for automobile lamps, which comprises the following components in parts by weight: 10-30 parts of 80000-5000000 mPas alkoxy-terminated 107 silicon rubber, 10-40 parts of 1000-80000 mPas alkoxy-terminated 107 silicon rubber, 30-50 parts of calcium powder, 1-10 parts of fumed silica, 1-10 parts of carbon paste, 1-5 parts of macromolecular crosslinking agent, 1-5 parts of coupling agent and 0.1-5 parts of catalyst. The invention also provides a preparation method of the anti-fog automobile lamp silicone sealant. The anti-fog automobile lamp silicone sealant disclosed by the invention has the advantages that the alkoxy end-capped 107 silicon rubber and the macromolecular crosslinking agent are used for replacing the traditional 107 silicon rubber and the single-molecule crosslinking agent, so that substances with destructive effects on an automobile lamp anti-fog coating are not generated in the curing and using processes. The invention relates to dealcoholized room temperature vulcanized organosilicon sealant, which is environment-friendly.
Chinese patent CN 111139023B provides a high-adhesion bi-component silicone sealant for vehicle lamps, comprising (7-12) by mass: a component A and a component B of the composition 1; the component A comprises 100 parts by weight of hydroxyl-terminated polydimethylsiloxane and 20-200 parts by weight of calcium carbonate, and the component B comprises 100 parts by weight of color paste, 5-40 parts by weight of cross-linking agent, 3-20 parts by weight of SC coupling agent and 1-15 parts by weight of catalyst; the SC coupling agent is prepared from the following raw materials: 5-50 parts of titanate compounds, 5-50 parts of aminosilicone and 50 parts of absolute ethyl alcohol.
Chinese patent CN 104877621B discloses an organosilicon sealant for vehicle lamp assembly and a preparation method thereof. The main components of the organic silicon sealant comprise active silicone oil or methyl silicone oil with the total mass content of the inactive organic silicon low molecular ring bodies D3-D10 being lower than 0.05%, reinforcing fillers such as white carbon black and calcium carbonate, cross-linking agents such as alkoxy silane or hydrogen-containing silicone oil with the total mass content of the inactive organic silicon low molecular ring bodies D3-D10 being lower than 0.05%, condensation or addition curing catalysts, modified silane coupling agent tackifier and the like. In addition, the organic silicon sealant has the characteristic that the total mass content of organic silicon low-molecular ring bodies D3-D10 is lower than 0.05%, and can inhibit the fog phenomenon of the car lamp when being applied to car lamp assembly.
However, the prior art suffers from one or more of the following problems:
(1) The used cross-linking agent has a complex structure and is not easy to purchase, special synthesis is often needed, the macromolecular structure of the special cross-linking agent determines that the synthesized cross-linking agent is a composition formed by substances with different molecular weight distribution, and the consistency of each batch is difficult to ensure due to the molecular weight and the molecular weight distribution, so that the prepared sealant has poor performance consistency.
(2) The content of residual siloxane rings in most of the alpha, omega-dihydroxypolydimethylsiloxane (107 glue) in the market exceeds 0.1 percent, and the residual siloxane rings slowly migrate out in the use process of the product, so that potential influence is caused on products bonded by the sealant, and the anti-fog coating is easy to lose effectiveness when the anti-fog coating is especially used for an anti-fog car lamp.
(3) The anti-fog effect is not obvious by reducing the content of siloxane ring bodies in 107 glue, because other volatile micromolecule results with silicon-alkoxy groups are easy to attach to the surface of the anti-fog coating along with the extension of the service time except D3-D10, and gradually form hydrogen bonds or react with the anti-fog coating or form a transparent hydrophobic film by condensation on the anti-fog coating, the occurrence of the conditions can change the hydrophilicity of the anti-fog coating, so that the anti-fog coating fails. Moreover, compared with hydrophobic D3-D10, the small molecules with the silicon-alkoxy groups are more easily adsorbed by the hydrophobic coating with hydroxyl groups on the surface, and the negative effect on the antifogging coating is not ignored.
(4) In the prior art, strong initial adhesion and high extrusion performance are difficult to ensure simultaneously, the production of automobile parts is particularly high in efficiency, more sealing glue is expected to be extruded from a rubber pipe in the same glue-extruding pressure in the same time, so that the glue-extruding period of a single automobile lamp is reduced, the air tightness test is carried out from the glue-extruding completion to the automobile lamp on a product line, only the time interval of less than 30min is needed, if the sealing glue has high extrusion performance, and enough initial adhesion is not available, the air tightness test result of the automobile lamp is disqualified.
(5) The single-component dealcoholized sealant in the prior art has a short shelf life, generally only 6 to 9 months, reduces the flexibility of customers on inventory management, and particularly aims at overseas customers, consumes a considerable part of shelf life in maritime time, thereby greatly reducing the applicability of products.
Disclosure of Invention
Therefore, aiming at least one technical problem existing in the prior art, the invention provides a storage-stable single-component dealcoholized organosilicon sealant composition and a preparation method thereof, and the organosilicon sealant composition has good bonding performance and improved shelf life.
The aim of the invention is achieved by the following technical scheme.
In a first aspect, the present invention provides a storage stable one-part dealcoholized silicone sealant composition, wherein the silicone sealant composition comprises: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, 80-120 parts by weight of calcium carbonate, 0-10 parts by weight of plasticizer, 0-5 parts by weight of pigment and 6-12 parts by weight of curing agent, wherein the curing agent comprises a mixture which is obtained by stirring and mixing (by weight ratio) an alcohol-removing cross-linking agent (5-7) and (1-4) and (0.1-0.8) of a catalyst and a polyamino silane oligomer for 30-60 min under the moisture-isolating condition.
In the organic silicon sealant composition, the use of the amino coupling agent is beneficial to improving the adhesive property of the sealant, however, the introduction of the amino group can lead to the shortening of the shelf life of the dealcoholized organic silicon sealant of the titanate system. The invention discovers that the organosilicon sealant composition can keep good adhesion performance to a wide range of substrates and has a shelf life of more than 12 months after the small molecular amino coupling agent is replaced by the polyamino silane oligomer and is mixed with the dealcoholization crosslinking agent and the titanate catalyst according to a certain proportion and then added.
The invention provides an organosilicon sealant composition, wherein the alpha, omega-dihydroxy polydimethylsiloxane is 107 glue, and the content of a siloxane ring body is below 0.1 weight percent.
In the invention, the siloxane ring is a D3-D10 siloxane ring. In some embodiments, the content of siloxane rings in the α, ω -dihydroxydimethicone may be 0.01 wt%, 0.02 wt%, 0.03 wt%, 0.04 wt%, 0.05 wt%, 0.08 wt%, or a combination thereof. For example, the content of the siloxane ring in the α, ω -dihydroxypolydimethylsiloxane is 0.08% by weight or less.
In the present invention, the α, ω -dihydroxy polydimethylsiloxane is 107 gums and the viscosity at 25 ℃ may be 20000 to 80000cps. Examples of alpha, omega-dihydroxy polydimethylsiloxanes suitable for use in the present invention include, but are not limited to: alpha, omega-dihydroxy polydimethylsiloxane commercially available from Jiangxi blue Starfire Silicone Co., ltd under the designations "P48V20000", "HP48V20000", "P48V80000" and "HP48V 80000".
The silicone sealant composition provided according to the present invention, wherein the present invention is not particularly limited to calcium carbonate, may employ any calcium carbonate known in the art, for example, the CCS-25 calcium carbonate available from Guangxi Huana New materials Co., ltd.
In the present invention, the amount of calcium carbonate may be 80 parts by weight, 90 parts by weight, 100 parts by weight, 110 parts by weight, 120 parts by weight or a range of its composition.
The silicone sealant composition according to the present invention, wherein a plasticizer may be added as needed, is not particularly limited, and any plasticizer known in the art, such as simethicone, may be used. Such plasticizers are either self-contained or commercially available.
When used, the plasticizer may be used in an amount of 1 to 10 parts by weight, preferably 2 to 8 parts by weight, more preferably 4 to 6 parts by weight.
The silicone sealant composition according to the present invention, wherein pigments may be added as needed, is not particularly limited, and any pigments known in the art, such as carbon black paste, may be used. Such pigments are either self-made or commercially available.
When used, the pigment may be used in an amount of 0.1 to 5 parts by weight, preferably 0.5 to 3 parts by weight, more preferably 1 to 3 parts by weight.
The organic silicon sealant composition provided by the invention, wherein the dealcoholized crosslinking agent is selected from methyltrimethoxysilane, vinyltrimethoxysilane, propyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethoxysilane, phenyltrimethoxysilane, 1, 2-bis trimethoxysilylethane and mixtures thereof.
The silicone sealant composition provided by the invention, wherein the catalyst is selected from titanate catalyst, titanate complex (chelate), dibutyl tin dilaurate, dibutyl tin diacetate and mixtures thereof. In some embodiments, the catalyst comprises a titanate complex or a mixture of a titanate complex and a titanate catalyst, the weight ratio of the titanate complex to the titanate catalyst in the mixture being from 1 to 5:1, such as from 1 to 3:1.
The silicone sealant composition provided by the invention, wherein the polyaminosilane oligomer can be a silane oligomer with 2-4 amino groups. Examples of polyaminosilane oligomers suitable for use in the present invention include, but are not limited to: number of marks isOligomeric bis-aminosilanes, aminosilane oligomer under the designation JH-AP1231, under the designationAmino silane of (a).
The weight ratio of the dealcoholization type cross-linking agent, the catalyst and the polyamino silane oligomer can be (5-6): 2-3): 0.2-0.6.
The organic silicon sealant composition provided by the invention, wherein the curing agent comprises a mixture obtained by stirring and mixing a dealcoholized cross-linking agent, a catalyst and a polyamino silane oligomer at the temperature of 20-30 ℃, preferably at room temperature under the condition of moisture isolation for 30-60 min.
The silicone sealant composition provided according to the present invention, wherein the stirring and mixing are performed at a stirring speed of 50 to 1000 rpm, preferably 100 to 500 rpm.
The silicone sealant composition provided by the invention can be used in an amount of 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, 10 parts by weight, 11 parts by weight, 12 parts by weight or a range consisting of the same.
In a second aspect, the present invention provides a method of preparing the one-part dealcoholized silicone sealant composition of the first aspect, wherein the method of preparing comprises the steps of:
s100, stirring and mixing a dealcoholized crosslinking agent, a catalyst and a polyamino silane oligomer with the weight ratio of (5-7) to (1-4) to (0.1-0.8) under the condition of moisture isolation to obtain a curing agent;
s200, stirring and mixing alpha, omega-dihydroxyl polydimethylsiloxane, calcium carbonate, optional plasticizer and optional pigment at the temperature of 120-160 ℃ and negative pressure of minus 0.085-minus 0.099MPa, and cooling to obtain premix;
s300, adding the curing agent prepared in the step S100 into the premix prepared in the step S200, and stirring and mixing under negative pressure of-0.085 to-0.099 MPa.
According to the preparation method provided by the invention, the stirring and mixing conditions in the step S100 comprise: the stirring speed is 50-1000 rpm, preferably 100-500 rpm; and/or at a temperature of 20 to 30 ℃, preferably at room temperature; and/or stirring and mixing for 30-60 min.
According to the preparation method provided by the invention, the stirring and mixing conditions in the step S200 comprise: the stirring speed is 100-1000 rpm, preferably 200-800 rpm; and/or the time is 60-180 min.
According to the preparation method provided by the invention, the temperature is cooled to room temperature in the step S200.
According to the preparation method provided by the invention, the stirring and mixing conditions in the step S300 comprise: the stirring speed is 100-1000 rpm, preferably 200-800 rpm; and/or the time is 30-60 min.
The invention has the following advantages: the organic silicon sealant composition provided by the invention has the advantages that through reasonable compounding, the obtained sealant product has high anti-fog effect, is well adhered to a base material, and has a shelf life exceeding 11 months, thereby meeting the high-speed glue spraying rate, ensuring enough initial adhesion, being capable of meeting the requirement of rapidly spraying glue on a car lamp production line, and passing the air tightness test after 20 minutes of glue spraying.
Detailed Description
The invention is further illustrated below with reference to specific examples.
The raw materials used in the examples and comparative examples are as follows:
(1) Alpha, omega-dihydroxy polydimethylsiloxane (107 gum)
| Number plate | Viscosity (cps) | D3-D10 content/wt% | Suppliers (suppliers) |
| H48V20000 | 20000 | 0.50 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
| H48V80000 | 80000 | 0.60 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
| P48V20000 | 20000 | 0.03 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
| P48V80000 | 80000 | 0.03 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
| HP48V20000 | 20000 | 0.03 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
| HP48V80000 | 80000 | 0.03 | JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. |
(2) Vinyl trimethoxy silane, industrial grade, hangzhou silicon chemical Co., ltd;
(3) Tetramethoxysilane, industrial grade, hangzhou silicon chemical Co., ltd;
(4) Number of marks isOligomeric bisaminosilanes of (a) and guangzhou firm with chemical industry import and export limited company;
(5) Number of marks isTitanate chelate of Guangzhou firm chemical industry import and export limited company;
(6) Titanium catalyst D60, hubei New blue sky New Material Co., ltd;
(7) Calcium carbonate: CCS-25, guangxi Huana New Material stock Co., ltd;
(8) Dimethicone: H47V100, jiangxi blue starfire silicone limited;
(9) Carbon black color paste: new materials limited, san francisco (Shanghai);
(10) KH550, KH792: ara Ding Huaxue reagent Co.
Example 1
(1) 6 parts by weight of vinyltrimethoxysilane, 3 parts by weight ofTitanate chelate and 0.2 part by weight ∈>The oligomeric bisaminosilane is stirred and mixed for 30min at room temperature under the condition of isolating moisture, so as to obtain the curing agent 1, wherein the stirring speed is 100 revolutions per min.
(2) Adding 40 parts by weight of P48V20000, 60 parts by weight of P48V80000 and 90 parts by weight of calcium carbonate CCS-25 into high-speed stirring equipment with a heating and vacuumizing system, uniformly dispersing, stirring for 180min at 120 ℃ and minus 0.085MPa, and cooling to room temperature to obtain the base adhesive 1, wherein the stirring speed is 500 revolutions per minute.
(3) Stirring the curing agent 1 and the base adhesive 1 for 50min under negative pressure of-0.095 MPa, discharging, and packaging to obtain the single-component dealcoholized organosilicon sealant composition, wherein the stirring speed is 500 revolutions per minute.
Example 2
The composition formulation and method of preparation were substantially the same as in example 1, except that: the step (1)The amount of oligomeric bisaminosilane was changed to 0.1 parts by weight.
Example 3
The composition formulation and method of preparation were substantially the same as in example 1, except that: the step (1)The amount of oligomeric bisaminosilane was changed to 0.6 parts by weight.
Example 4
The composition formulation and method of preparation were substantially the same as in example 1, except that: the step (1)The amount of oligomeric bis-aminosilane was changed to 0.8 parts by weight.
Comparative examples 1 to 1
The composition formulation and method of preparation were substantially the same as in example 1, except that: the step (1)The oligomeric bis-aminosilane was changed to KH550 in the same parts by weight.
Comparative examples 1 to 2
The composition formulation and method of preparation were substantially the same as in example 1, except that: 0.2 part by weight of the catalyst in the step (1)The oligomeric bis-aminosilane was changed to 0.8 parts by weight of KH550.
Comparative examples 1 to 3
The composition formulation and method of preparation were substantially the same as in example 1, except that: step (1) is not performed, and 6 parts by weight of vinyltrimethoxysilane and 3 parts by weight of the catalyst are directly added in step (3)Titanate chelate and 0.2 part by weight ∈>Adding oligomeric bisaminosilane into the base adhesive 1, stirring for 50min under negative pressure of-0.095 MPa, discharging, and packaging.
Comparative examples 1 to 4
The composition formulation and method of preparation were substantially the same as in example 1, except that: the mark in the step (1) is given asThe same weight parts of KH792 was used instead of the oligomeric bis-aminosilane.
Comparative examples 1 to 5
The composition formulation and method of preparation were substantially the same as in example 1, except that: the amount of vinyltrimethoxysilane used in step (1) was changed to 8 parts by weight.
Comparative examples 1 to 6
The composition formulation and method of preparation were substantially the same as in example 1, except that: the amount of vinyltrimethoxysilane used in step (1) was changed to 3 parts by weight.
Comparative examples 1 to 7
The composition formulation and method of preparation were substantially the same as in example 1, except that: the step (1)The amount of oligomeric bisaminosilane was changed to 0.05 parts by weight.
Example 5
(1) 5 parts by weight of methyltrimethoxysilane, 2 parts by weightTitanate chelate, 1 part by weight of titanium catalyst D60 and 0.5 part by weight of ∈>The oligomeric bisaminosilane was mixed at room temperature with moisture exclusion for 30min to give curing agent 2, wherein the stirring speed was 100 revolutions per minute.
(2) 50 parts by weight of HP48V20000, 50 parts by weight of HP48V80000, 5 parts by weight of simethicone H47V100, 3 parts by weight of carbon black color paste and 110 parts by weight of calcium carbonate CCS-25 are added into high-speed stirring equipment with a heating and vacuumizing system, uniformly dispersed, stirred for 120min at 120 ℃ under minus pressure of-0.092 MPa, cooled to room temperature, and base rubber 2 is obtained, wherein the stirring speed is 500 revolutions per minute.
(3) Stirring the curing agent 2 and the base adhesive 2 for 60min under negative pressure of-0.095 MPa, discharging, and packaging to obtain the single-component dealcoholized organosilicon sealant composition, wherein the stirring speed is 500 revolutions per minute.
Example 6
The composition formulation and method of preparation were substantially the same as in example 5, except that: in the step (1)The amount of titanate chelate is reduced from 2 parts by weight to 1 part by weight.
Comparative example 2-1
The composition formulation and method of preparation were substantially the same as in example 5, except that: the amount of methyltrimethoxysilane in step (1) was changed to 10 parts by weight.
Comparative examples 2 to 2
The composition formulation and method of preparation were substantially the same as in example 5, except that: the amount of methyltrimethoxysilane in step (1) was changed to 8 parts by weight.
Comparative examples 2 to 3
The composition formulation and method of preparation were substantially the same as in example 5, except that: the amount of methyltrimethoxysilane in step (1) was changed to 3 parts by weight.
Comparative examples 2 to 4
The composition formulation and method of preparation were substantially the same as in example 5, except that: the dosage of the simethicone in the step (2) is changed to 30 parts by weight.
Comparative examples 2 to 5
The composition formulation and method of preparation were substantially the same as in example 5, except that: the amount of calcium carbonate CCS-25 used in step (2) was changed to 130 parts by weight.
Performance testing
1. The compositions of the examples and comparative examples were subjected to the relevant tests according to the following criteria:
the surface dry time is tested according to GB/T13477;
tensile strength was measured according to GB/T528 (type 2 test specimen);
elongation at break was measured according to GB/T528 (type 2 test specimen);
hardness was measured according to GB/T531.
2. Extrusion rate test method:
the 300mL gum bottle with 3mm tip is placed under a pneumatic device with 0.3MPa pressure, the weight of gum passing through the tip in unit time is measured, each sample is tested 3 times, the extrusion time is 15s each time, and the median value is taken according to g/min.
3. The air tightness test method comprises the following steps:
and placing the car lamp box cover just after the glue is sprayed on the production line at room temperature for 20min, then placing the car lamp box cover in an A601 type air tightness leak detector for detection, wherein the air pressure is 18kPa, the air is inflated for 10 seconds, the balance is carried out for 10 seconds, the detection is carried out for 5 seconds, the air is deflated for 3 seconds, and the leak rate is less than 30Pa, so that the car lamp box cover is qualified.
4. Adhesion test:
and wiping the parts, which are required to be adhered, of the car lamp with ethanol at the temperature of 23 ℃ and in the humidity of 50% RH, standing for 30min to volatilize the ethanol completely, uniformly coating the sealant to the thickness of about 3mm, curing for 14d, and observing the adhesion strength of the sealant to the car lamp according to three standard grades of excellent, medium and poor.
5. The anti-fog effect testing method comprises the following steps:
1) Gluing about 50g in a surface dish, and uniformly spreading;
2) Placing a flat and transparent substrate coated with an anti-fog coating on a surface dish, enabling the surface with the anti-fog coating to face downwards, sealing the surface with the anti-fog coating in a self-sealing bag together, and enabling small molecules released by the organosilicon sealant in the curing process to fully contact with the anti-fog coating;
3) After the sealant is solidified for 72 hours, the surface dish and the transparent substrate coated with the anti-fog coating are treated for 24 hours in the environment of 80 ℃, and cooled to 23+/-2 ℃;
4) Placing the treated transparent substrate above warm water at 80 ℃, observing for 30 seconds, judging whether the part of the transparent substrate coated with the anti-fog coating is transparent or fog-changing, scoring according to subjective judgment, giving 5 points when the transparent substrate is completely transparent, giving 0 points when the transparency is lower, evaluating by three persons randomly, and taking the median value.
6. The quality guarantee period testing method comprises the following steps:
placing the sample under the conditions of 23+/-2 ℃ and 50+/-5% RH, storing in a dark place, measuring the tensile strength and the hardness of the sample once every month, and judging the sample to be in the quality guarantee period when the two indexes are kept above 60% of the original indexes; and otherwise, judging that the quality guarantee period is exceeded.
Table 1 properties of the examples and comparative compositions
As can be seen from table 1, example 1 meets the requirements of air tightness test, adhesive property, anti-fog property and shelf life at the same time; in comparative example 1-1, the amino coupling agent is replaced, so that the adhesion performance to the car lamp is insufficient, and the shelf life is shortened; comparative examples 1-2 increased the amount of KH550, improved adhesion, but severely shortened shelf life; the cross-linking agent, amino coupling agent and catalyst of comparative examples 1-3 were not pretreated, and the shelf life of the product was significantly shortened compared to example 1; comparative examples 1-4 replaced coupling agent KH792, while improving adhesion, affecting tack-free time and shelf life; comparative examples 1-5 have an excessive amount of crosslinking agent and have a lower antifogging effect than example 1; the cross-linking agent in comparative examples 1-6 is too little, the glue making process is seriously thickened, and the glue cannot be normally discharged; the comparative examples 1 to 7 were poor in adhesion to the lamp due to too small an amount of the polyaminosilane oligomer; examples 1 and 3, in which the amount of the polyamino silane oligomer used was 0.2 parts by weight and 0.6 parts by weight, were excellent in combination properties, and example 2, in which the amount of the polyamino silane oligomer used was reduced, had a certain improvement in adhesion to a vehicle lamp, but in example 4, when the amount of the polyamino silane oligomer used was relatively large, the antifogging effect and shelf life were rather lowered.
As can be seen from table 1, examples 5 and 6 have good overall properties; the dosage of the cross-linking agent in comparative example 2-1 is too much, and the antifogging effect is obviously reduced; comparative example 2-2 slightly reduced the amount of crosslinker (still excessive), improved the anti-fog effect, but not as in example 5; in comparative examples 2 to 3, the amount of the cross-linking agent is too small, so that the glue is seriously thickened in the glue making process, and the glue cannot be normally discharged; comparative examples 2-4, though increasing the extrusion rate by increasing the amount of plasticizer, resulted in failure of the air tightness test; the comparative examples 2-5 increased the amount of calcium carbonate, although the performances such as air tightness, anti-fog, etc. met the use requirement, but the extrusion rate was too low, which resulted in a slow glue-making speed of the production line, affecting the production efficiency, and simultaneously the hardness was too high after curing, which was unfavorable for shock absorption.
According to the data of the comprehensive embodiment, the organosilicon sealant composition provided by the invention has the advantages that through a reasonable formula, the obtained sealant product has more excellent anti-fog effect, is well adhered to a base material, has a shelf life exceeding 11 months, meets the high-speed sealant-beating rate, ensures enough initial adhesion, can meet the requirement of quick sealant beating of a car lamp production line, and can pass the air tightness test 20min after sealant beating.
Claims (10)
1. A storage stable one-part dealcoholized silicone sealant composition, wherein the silicone sealant composition comprises: 100 parts by weight of alpha, omega-dihydroxy polydimethylsiloxane, 80-120 parts by weight of calcium carbonate, 0-10 parts by weight of plasticizer, 0-5 parts by weight of pigment and 6-12 parts by weight of curing agent, wherein the curing agent comprises a mixture which is obtained by stirring and mixing (by weight ratio) an alcohol-removing cross-linking agent (5-7) and (1-4) and (0.1-0.8) of a catalyst and a polyamino silane oligomer for 30-60 min under the moisture-isolating condition.
2. The silicone sealant composition according to claim 1, wherein the content of siloxane rings in the α, ω -dihydroxypolydimethylsiloxane is 0.1 wt.% or less, preferably 0.08 wt.% or less;
and/or the alpha, omega-dihydroxy polydimethylsiloxane has a viscosity of 20000 to 80000cps at 25 ℃.
3. The silicone sealant composition according to claim 1 or 2, wherein the plasticizer is used in an amount of 1 to 10 parts by weight, preferably 2 to 8 parts by weight, more preferably 4 to 6 parts by weight;
and/or the plasticizer is dimethyl silicone oil.
4. A silicone sealant composition according to any one of claims 1-3, wherein the pigment is used in an amount of 0.1-5 parts by weight, preferably 0.5-3 parts by weight, more preferably 1-3 parts by weight.
5. The silicone sealant composition of any of claims 1-4 wherein the dealcoholized crosslinking agent is selected from methyltrimethoxysilane, vinyltrimethoxysilane, propyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethoxysilane, phenyltrimethoxysilane, 1, 2-bis trimethoxysilylethane, and mixtures thereof;
and/or the catalyst is selected from titanate catalysts, titanate complexes, dibutyltin dilaurate, dibutyltin diacetate, and mixtures thereof;
and/or the polyaminosilane oligomer is a silane oligomer having 2-4 amino groups.
6. The silicone sealant composition of claim 5 wherein the polyaminosilane oligomer is selected from the group consisting of the trade names @1146 oligomeric bis-aminosilanes, aminosilane oligomer under the designation JH-AP1231 and aminosilane oligomer under the designation JH-AP1231Amino silane of SIVO 203.
7. The silicone sealant composition of any of claims 1-6 wherein the weight ratio of the dealcoholized crosslinking agent, the catalyst, and the polyaminosilane oligomer is (5-6): 2-3): 0.2-0.6.
8. The silicone sealant composition according to any one of claims 1-7, wherein the curing agent comprises a mixture obtained by mixing a dealcoholized crosslinking agent, a catalyst and a polyaminosilane oligomer with stirring at a temperature of 20-30 ℃, preferably at room temperature, under moisture-proof conditions for 30-60 min.
9. A method of preparing the silicone sealant composition of any of claims 1-18, wherein the method of preparing comprises the steps of:
s100, stirring and mixing a dealcoholized crosslinking agent, a catalyst and a polyamino silane oligomer with the weight ratio of (5-7) to (1-4) to (0.1-0.8) under the condition of moisture isolation to obtain a curing agent;
s200, stirring and mixing alpha, omega-dihydroxyl polydimethylsiloxane, calcium carbonate, optional plasticizer and optional pigment at the temperature of 120-160 ℃ and negative pressure of minus 0.085-minus 0.099MPa, and cooling to obtain premix;
s300, adding the curing agent prepared in the step S100 into the premix prepared in the step S200, and stirring and mixing under negative pressure of-0.085 to-0.099 MPa.
10. The silicone sealant composition according to claim 9, wherein the conditions of stirring and mixing in step S100 include: the stirring speed is 50-1000 rpm, preferably 100-500 rpm; and/or at a temperature of 20 to 30 ℃, preferably at room temperature; and/or stirring and mixing for 30-60 min;
and/or, the conditions of stirring and mixing in step S200 include: the stirring speed is 100-1000 rpm, preferably 200-800 rpm; and/or, the time is 60-180 min;
and/or, the conditions of stirring and mixing in step S300 include: the stirring speed is 100-1000 rpm, preferably 200-800 rpm; and/or the time is 30-60 min.
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| CN202311176102.4A CN117186832A (en) | 2023-09-13 | 2023-09-13 | Storage-stable one-component dealcoholized organosilicon sealant composition and preparation method thereof |
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